CN114551811A - Preparation method of vertical MXene array pole piece, vertical MXene array pole piece and application - Google Patents
Preparation method of vertical MXene array pole piece, vertical MXene array pole piece and application Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a preparation method of a vertical MXene array pole piece, and belongs to the technical field of batteries. The preparation method comprises the following steps: preparing MXene nano-sheets and preparing a vertical MXene array pole piece; dispersing MXene nanosheet powder to prepare a dispersion liquid to obtain an MXene dispersion liquid; cutting copper foil and placing on a freezing plate; placing MXene dispersion liquid on a copper foil and coating, wherein the coating thickness is 50-500 micrometers; and after coating is finished, freeze-drying to obtain the vertical MXene array pole piece. The preparation method provided by the invention designs the MXene nanosheets into a vertical three-dimensional structure by using an ice template method, can effectively utilize all MXenes, can form a uniform and vertical SEI layer on the surface of the vertical MXene in the reaction process with Li, effectively reduces the side reaction of metal lithium and electrolyte, and has good performance when being used as a lithium metal cathode.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a preparation method of a vertical MXene array pole piece, the vertical MXene array pole piece prepared by the preparation method of the vertical MXene array pole piece and application of the vertical MXene array pole piece as a negative electrode of a lithium metal battery.
Background
MXene material is a kind of metal carbon/nitride with two-dimensional layered structure and its chemical general formula is Mn+1XnTXWherein (n ═ 1-3), M represents an early transition metal such as Ti, Zr, V, Mo, etc.; x represents a C or N element, Tx is a surface group, typically-OH, -O, -F and-Cl. It is known as MXene because of its lamellar structure similar to Graphene.
The lithium metal battery is a battery using metal lithium as a negative electrode, and the capacity of the lithium battery can be greatly increased by using the metal lithium as a negative electrode material of the lithium battery instead of graphite, and is one of the most promising next-generation high energy density storage devices. However, lithium metal has extremely active chemical properties, and besides, the lithium metal also has problems of growth of lithium dendrite and volume expansion during charge and discharge cycles, which greatly hinders the development of lithium metal batteries. Due to the intrinsic thermodynamic instability of lithium metal, non-uniform lithium plating/stripping and uncontrolled side reactions can result, which in turn can lead to the growth of lithium dendrites and the formation of a brittle natural Solid Electrolyte Interphase (SEI), which can induce loss of active material and internal shorting, greatly limiting the commercial application of lithium metal negative electrodes. In order to solve this problem, a commonly used solution is to use a three-dimensional electrode material. On one hand, the three-dimensional structure provides enough space and a stable frame structure for lithium ion deposition, and the problem of infinite volume change can be solved; on the other hand, the pore channel structure provides a larger surface area, so that the local surface current density is effectively reduced, and the effect of uniformly distributing lithium ion flux is achieved, so that the generation of lithium dendrite is reduced.
The commonly used three-dimensional electrode materials are mainly three-dimensional carbon materials (raw materials are graphene, carbon nanotubes, carbon fibers and the like) and three-dimensional metal materials (foamed nickel, foamed copper and the like). Carbon-based materials have the advantages of low density, high surface area, high conductivity, adjustable characteristics, inexpensive and ubiquitous precursors, and well-known simple chemical methods, and can be used to produce the latest structures suitable for lithium metal cathodes with adjustable physicochemical properties. Metal-based electrode materials (including conducting or non-conducting metal compounds and alloys thereof) can direct uniform Li metal deposition in a variety of ways, for example, through the formation of highly Li-ion conducting layers, the formation of thiophilic compounds, the induction of active nucleation sites and the formation of nanopores with structural and effective surface area expansion.
However, the three-dimensional metal material itself has a large weight, which results in a low specific energy of the entire battery. With the three-dimensional carbon material, the carbon material itself is limited in further improvement of battery performance due to the lack of metal lithium deposition sites and the unprotected interface between the lithium metal and the electrolyte.
Disclosure of Invention
In view of the above, in order to solve the technical problems of dendritic growth, infinite volume change, large mass of a lithium metal negative electrode with a three-dimensional structure and lack of active sites of the lithium metal negative electrode of a lithium metal battery, the invention provides a preparation method of a vertical MXene array pole piece on one hand, wherein an ice template method is used for designing an MXene nanosheet into a vertical three-dimensional structure, all MXenes can be effectively utilized, and a uniform and vertical SEI layer can be formed on the surface of the vertical MXene in the reaction process with Li, so that the side reaction of metal lithium and electrolyte can be effectively reduced, and the vertical MXene array pole piece has good performance as the lithium metal negative electrode.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a vertical MXene array pole piece comprises the following steps:
1) preparation of MXene nanosheets:
etching, centrifuging, washing, drying and ultrasonically dispersing MAX powder under the action of hydrochloric acid and lithium fluoride to obtain MXene nanosheet solution, and then freeze-drying to finally obtain MXene nanosheet powder;
2) preparing a vertical MXene array pole piece:
21) dispersing the MXene nanosheet powder to prepare a dispersion liquid to obtain an MXene dispersion liquid;
22) cutting copper foil and placing on a freezing plate;
23) placing the MXene dispersion liquid on the copper foil and coating, wherein the coating thickness is 50-500 micrometers;
24) and after coating is finished, freeze-drying to obtain the vertical MXene array pole piece.
Preferably, the MAX powder is Ti3AlC2、Ti2AlC、V2One kind of AlC.
Preferably, the mass volume ratio of the lithium fluoride to the hydrochloric acid is (5-10) g: (100-200) ml, wherein the mass ratio of the MAX powder to the lithium fluoride is (4-10): (5-10), wherein the concentration of the hydrochloric acid is 6-12 mol/L.
Preferably, the etching time is 24-48 hours;
the rotating speed of the centrifugation is (2500-.
Preferably, the concentration of the MXene nanosheet solution is 0.25-2 mg/ml.
Preferably, the concentration of the MXene dispersion is 50mg to 150 mg/ml.
Preferably, the freezing temperature of the freezing plate is from-60 ℃ to-20 ℃.
Preferably, 24), the freeze-drying time is 24 hours, and the freeze-drying air pressure is less than 30 pa.
On the other hand, the invention also provides the vertical MXene array pole piece prepared by the preparation method.
On the other hand, the invention also provides application of the vertical MXene array pole piece as a lithium metal battery cathode.
Compared with the prior art, the invention has the following beneficial effects:
the MXene nanosheets are designed into a vertical three-dimensional structure by using an ice template method, all MXenes can be effectively utilized, and a uniform and vertical SEI layer can be formed on the surface of the vertical MXene in the reaction process with Li, so that the side reaction of metal lithium and electrolyte can be effectively reduced, and the MXene nanosheets have good performance when being used as a lithium metal cathode;
MXene materials have O-containing and F-containing functional groups per se, and can serve as Li-philic sites. The commonly used electrode is composed of horizontally stacked MXene nanosheets, which enables only the MXene surface of the uppermost layer to participate in metal lithium deposition, resulting in large local current density and non-uniform lithium deposition.
Drawings
Fig. 1 is an XRD pattern of MXene nanoplatelets;
fig. 2 is a TEM image of MXene nanoplates;
FIG. 3 is an AFM image of MXene nanoplatelets;
FIG. 4 is a schematic diagram of the preparation of a vertical MXene array pole piece;
FIG. 5 is a SEM image of one of the vertical MXene array pole pieces;
FIG. 6 is another SEM image of a vertical MXene array pole piece;
FIG. 7 is a cross-sectional SEM image of a vertical MXene array pole piece;
FIG. 8 is an EDS-Mappinig test chart;
FIG. 9 shows that the deposition capacity of the vertical MXene negative electrode is 6mAh/cm2SEM image of metal Li of (a), right side is a sectional view;
FIG. 10 shows that the horizontal MXene electrode deposition capacity is 6mAh/cm2SEM image of metal Li of (a), right sectional view;
FIG. 11 shows 1mAh/cm2、1mA/cm2A vertical MXene and horizontal MXene half-cell cycle performance diagram under the parameters;
Detailed Description
As shown in fig. 1 to 9, the present invention provides a method for preparing a vertical MXene array pole piece, comprising the following steps:
1) preparation of MXene nanosheet:
etching, centrifuging, washing, drying and ultrasonically dispersing MAX powder under the action of hydrochloric acid and lithium fluoride to obtain MXene nanosheet solution, and freeze-drying the obtained MXene nanometer solution to finally obtain MXene nanosheet powder;
wherein the MAX powder is Ti3AlC2、Ti2AlC、V2One of AlC;
wherein the mass volume ratio of the lithium fluoride to the hydrochloric acid is (5-10) g: (100-200) ml, wherein the mass ratio of MAX powder to lithium fluoride is (4-10): (5-10) the concentration of hydrochloric acid is 6-12 mol/L
Wherein, the etching time is 24-48 hours, the centrifugation rotation speed is (2500-;
wherein the concentration of the MXene nanosheet solution is 0.25-2 mg/ml;
2) preparing a vertical MXene array pole piece:
prepared MXene nanosheet powder (Ti) is adopted3C2、Ti2C、V2C) is dispersed by water to prepare MXene dispersion liquid with the concentration of 50mg-150 mg/ml;
cutting a piece of copper foil (the preferred thickness is 100 microns, the length and the broadband are cut according to the requirements, the preferred length is 20cm, the preferred width is 10cm) according to the requirements, placing the copper foil on a freezing plate (the preferred freezing temperature is 60 ℃ below zero to 20 ℃ below zero), and cooling the freezing plate by liquid nitrogen;
placing the MXene dispersion on a copper foil and coating with a height-adjustable doctor blade (preferably 50-500 μm thick); the height of the synthesized vertical MXene array pole piece can be adjusted by adjusting the height of the scraper;
in the coating process, the MXene nanosheets are also arranged in the vertical direction along with the icing action of water in the vertical direction;
and after the completion, freeze-drying the coated pole piece in a freeze-drying machine, preferably for 24 hours, preferably under the freeze-drying pressure of less than 30pa, and obtaining the vertical MXene array pole piece after the freeze-drying is finished.
The invention also provides the vertical MXene array pole piece prepared by the preparation method and application of the pole piece as a negative electrode of a lithium metal battery.
FIG. 2 shows that the MXene nanosheet has a platelet diameter of 3-10 um; FIG. 3 shows MXene nanosheets having a thickness of 3-5 nm; FIG. 8 shows that the O and F elements are distributed along the array; as shown in fig. 9, it can be seen that metallic lithium fills the entire three-dimensional vertical skeleton and is deposited flat;
the technical scheme of the invention is explained in detail below by combining with specific embodiments, and the vertical MXene array pole piece is prepared by using the preparation method.
Example 1
The technological parameters are controlled as follows:
Ti3AlC24g, 10g of lithium fluoride, 6mol/L of hydrochloric acid with the volume of 100ml, 24 hours of etching time, 3000rpm of centrifugation, 10 minutes of centrifugation, repeating for multiple times until the PH of the solution is 6 to obtain the MXene nanosheet solution with the concentration of 4 mg/ml;
the concentration of MXene dispersion is 50mg/ml, the length of copper foil is 100 microns, the freezing temperature is minus 40 ℃, the coating is 50 microns, the freeze-drying time is 24 hours, and the freeze-drying air pressure is 15 pa.
Example 2
The technological parameters are controlled as follows:
Ti3AlC24g, 10g of lithium fluoride, 6mol/L of hydrochloric acid with the volume of 100ml, 24 hours of etching time, 3000rpm of centrifugation, 10 minutes of centrifugation, repeating for multiple times until the PH of the solution is 6 to obtain 2mg/ml of MXene nanosheet solution;
the concentration of MXene dispersion is 100mg/ml, the length of copper foil is 100 micrometers, the freezing temperature is minus 40 ℃, the coating is 50 micrometers, the freeze-drying time is 24 hours, and the freeze-drying air pressure is 20 pa.
Example 3
The technological parameters are controlled as follows:
Ti3AlC24g, 10g of lithium fluoride, 6mol/L of hydrochloric acid with the volume of 100ml, 24 hours of etching time, 3000rpm of centrifugation, 10 minutes of centrifugation, repeating for multiple times until the PH of the solution is 6 to obtain the MXene nanosheet solution with the concentration of 4 mg/ml;
the concentration of MXene dispersion is 150mg/ml, the length of copper foil is 100 microns, the freezing temperature is minus 20 ℃, the coating is 100 microns, the freeze-drying time is 24 hours, and the freeze-drying air pressure is 20 pa.
Example 4
The technological parameters are controlled as follows:
Ti2AlC8g, lithium fluoride 10g, hydrochloric acid concentration 9mol/L volume 100ml, etching time 48 hours, centrifugal rotation speed 3000rpm, centrifugal time 10min, repeating for multiple times until the PH of the solution is 7 to obtain MXene nanosheet solution with concentration of 1 mg/ml;
the concentration of MXene dispersion is 100mg/ml, the length of copper foil is 100 micrometers, the freezing temperature is minus 40 ℃, the coating is 150 micrometers, the freeze-drying time is 24 hours, and the freeze-drying air pressure is 25 pa.
Example 5
The technological parameters are controlled as follows:
V210g of AlC10g, 10g of lithium fluoride, 12mol/L of hydrochloric acid, 150ml of volume, 24 hours of etching time, 2000rpm of centrifugation speed and 10min of centrifugation time, and repeating the steps until the PH of the solution is 8 to obtain 1mg/ml of MXene nanosheet solution;
the concentration of MXene dispersion liquid is 200mg/ml, the length of copper foil is 100 micrometers, the freezing temperature is 60 ℃ below zero, the coating is 100 micrometers, the freeze-drying time is 24 hours, and the freeze-drying air pressure is 25 pa.
Battery assembly testing
The button cell is assembled by respectively adopting the vertical MXene array pole pieces prepared in the embodiments 1-5 as negative pole materials and the horizontal MXene negative pole as a comparative example, and the battery performance test is carried out by the following specific method:
the battery performance testing process comprises the following steps:
the obtained vertical MXene array pole piece is directly cut into a vertical MXene array electrode negative pole piece with the radius of 10 mm.
Preparing a horizontal MXene pole piece, namely stirring MXene powder and a binder in a proper amount of N-methyl-2-pyrrolidone for 3-4 h according to the mass ratio of 4:1 during assembling of the battery, uniformly mixing, transferring and coating the uniformly mixed black slurry on a copper foil, and performing vacuum drying at 85 ℃ for 12 h. The coated copper foil is cut into a negative electrode piece with the radius of 10mm, a lithium metal sheet is used as a reference electrode and a counter electrode, a mesoporous polypropylene film is used as a diaphragm (Celgard2400), 40 mu L of mixed solution of 1, 3-Dioxolane (DOL) and methylal (DME) dissolved with 1M lithium bis (trifluoromethyl sulfonyl) imide (LiTFSI) and 2% LiNO3 is added as electrolyte, a C2025 button cell is assembled in a glove box, and argon is filled in the glove box to ensure that the content of water and oxygen is less than 0.1 ppm. After the assembly is completed, the battery is subjected to constant current charge and discharge test by using the Xinwei battery test system.
And (3) testing conditions are as follows: firstly, 0.05mA cm is used-2The current density of the lithium ion battery is activated for five circles within a voltage interval of 0.01-1V, then lithium deposition is carried out at different current densities and times, then the voltage is increased to 1V for lithium removal, and a cycle test is carried out by taking the voltage as a period, and the result is that
As shown in fig. 10, it can be seen that lithium is deposited on the upper surface of the electrode, and is accompanied by the growth of lithium dendrites;
the performance of both is shown for example in fig. 11, where vertical MXene has better cycle performance than horizontal MXene, the coulombic efficiency of example 2, which is the best performance, is still 98.8% after 450 cycles, and the horizontal MXene is only 98.2% after 150 cycles.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (10)
1. A preparation method of a vertical MXene array pole piece is characterized by comprising the following steps:
1) preparation of MXene nanosheets:
etching, centrifuging, washing, drying and ultrasonically dispersing MAX powder under the action of hydrochloric acid and lithium fluoride to obtain MXene nanosheet solution, and then freeze-drying to finally obtain MXene nanosheet powder;
2) preparing a vertical MXene array pole piece:
21) dispersing the MXene nanosheet powder to prepare a dispersion liquid to obtain an MXene dispersion liquid;
22) cutting copper foil and placing on a freezing plate;
23) placing the MXene dispersion liquid on the copper foil and coating, wherein the coating thickness is 50-500 micrometers;
24) and after coating is finished, freeze-drying to obtain the vertical MXene array pole piece.
2. The method for preparing the vertical MXene array pole piece of claim 1, wherein the MAX powder is Ti3AlC2、Ti2AlC、V2One kind of AlC.
3. The method for preparing the vertical MXene array pole piece according to claim 1, wherein the mass volume ratio of the lithium fluoride to the hydrochloric acid is (5-10) g: (100-200) ml, wherein the mass ratio of the MAX powder to the lithium fluoride is (4-10): (5-10), wherein the concentration of the hydrochloric acid is 6-12 mol/L.
4. The method for preparing the vertical MXene array pole piece according to claim 1, wherein the etching time is 24-48 hours;
the rotating speed of the centrifugation is (2500-.
5. The method for preparing the vertical MXene array pole piece according to claim 1, wherein the concentration of the MXene nanosheet solution is 0.25-2 mg/ml.
6. The method for preparing the vertical MXene array pole piece according to claim 1, wherein the concentration of the MXene dispersion is 50mg-150 mg/ml.
7. The method for preparing a vertical MXene array pole piece as claimed in claim 1, wherein the freezing temperature of the freezing plate is from-60 ℃ to-20 ℃.
8. The method for preparing a vertical MXene array sheet according to any one of claims 1-7, wherein in 24), the freeze-drying time is 24 hours, and the freeze-drying pressure is less than 30 pa.
9. The vertical MXene array pole piece prepared by the preparation method of the vertical MXene array pole piece according to any one of claims 1-8.
10. Use of the vertical MXene array pole piece of claim 9 as a negative electrode for lithium metal batteries.
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| CN114944489A (en) * | 2022-06-15 | 2022-08-26 | 北京航空航天大学 | Thin film layer with accordion MXene array and preparation method thereof, current collector, electrode and battery |
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